FR2654116A1 - SPECTROCHEMICAL ANALYSIS CALIBRATION BY OPTICAL EMISSION FOR METALS AND ALLOYS. - Google Patents

Abstract

The invention relates to a standard for spectrochemical analysis by optical emission for metals and alloys. - The object of the invention is a standard for spectrochemical analysis by optical emission for metals and alloys, characterized in that it consists of a molten mixture of small metal bodies. The latter are advantageously obtained by rapid solidification and subjected to plastic deformation. - Application to the spectrochemical analysis of metals and alloys.

Description

A 49% of the total weight of a UI

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  the standard sample by chemical analysis.

  In optical emission spectrometry, the surface of such a standard sample is machined to be united, and then a calibration curve is established on the basis of a spectral intensity ratio caused by sparks generated in locations However, a segregation often occurs during the solidification of the molded metal, as is usual, if a large amount of alloying elements are contained. As a result, the spectral intensity varies depending on the difference locations, in a two-dimensional or three-dimensional space, of the surface exposed to sparks and, therefore, an exact analysis is impossible with such a standard sample In view of the foregoing, in order to reduce segregation at the solidification of the molten metal, the latter can sometimes be cast according to an ingot in the form of

  small diameter rod by a semicircle casting process

  continuous, then cut into a disc shape.

  However, the segregation can not be avoided even if the casting is carried out according to a rod-shaped ingot of small diameter and, in particular, the segregation becomes even more remarkable as the content of the element is increased. For example, in the case of alloys of the Al-Si series containing silicon exceeding a eutectic point, the primary crystals of silicon precipitate and the segregation of such precipitated primary crystals of silicon renders the calibration curve and the associated drift correction inaccurate, even if it is a casting according to a rod-shaped ingot, which does not allow

  not to make an exact analysis of the sample to be analyzed.

  Therefore, an object of the present invention is to overcome the problems mentioned above and to achieve a spectrochemical standard for optical emission analysis for metals and alloys, capable of allowing the establishment of a precise calibration curve and to make a correction

exact drift.

  The authors of the present invention have made various studies to overcome the above problems and have finally found that a standard for spectrochemical analysis is one of the most important tools in the world. quos sli T, nbsind 'ap To P Uo Tq Do TTPTF Ios ap snstea Dod a uo Ias saiedaid que sanb Tileam sd Io D sal Ts' no ua Aaq Dexx aa Tuew ap aes Amee Y J 4 ned Uo T Tt Bt Da I ap squaw, gi sep aneual Sú el anb aaos ua 'a Iq Tssod qsa as TDG-Id A-lap ap uo I Daj IOD aun -a as T Daid abeuuolqg, p aqano D au anbçrdo uo Tss Tma e Ta J 9 mwol Doads jed jaiedaid qnad uo 'a Duanbasuo D ua suo Tsuaw Tp se sael suep s TI Jadea S 4 uawa D Beduia sap L BITTI aipu Tow uo T 1 qbgaa 6 S aun au Qubomoq uolp 49 uo Il Tl Tuq Da a ian Tqsuo DO ú qua Anad ls ls Xuu, pa Dejans l y alqasua S ual su p s I tap I tap tos TD-xne Of sanb TI Law sdcoo sel Glua uo T 4 ef Jab 6 S tate ss w ow s ssl his 6 ue 19 WU OS s Itlnbs Tnld la alu Be, pa Dejins wl ais sanbi T Ti 4 gm sdao D xnaaqwou ap alodwo D anbll eqg sdioz D A, p Jf Jied e snssap-t D 4 a Dgop SZ awwo D anqfsuo D uoluq uol II Tuet Dal I anbs Tnd'Dq 'a Tm ITJ' ab F 4 'aliila T j' nl Bea Bo W 'su J 6 lb' at TJ 8 apn Iod a BT u 151 s UO-i Ue AUT aquasaid e T suep ,, anb I Teqigw sdo D ",, uo Issaldxal sagnb Tidxa suos Tei salt anod anbïqseld uo Tqi Logap ied jaeadaad oz el ap aoe; D Ja snld 4 sa IF se Bw Js Bal S Ui B a Belnow ap sapp Doid ap i Tqa 4 Ld g, amog alq 4 nad alnom abu Blpm a B 'snhd aa sgade-TD saq Tîaap suos Tea sa B anod ap Tdea uo Tt D Tj Tp Tios i Jd / a Bedgld at T ap B From DJ sn I Ld 4 s G IF s F We an Sn apa Dooid a jue aiedaid aeaq -nad anbf Ii Teqaw sdlo D aq sanb Tiie Tau sdloo sq Tad ap 9 Ino L abuelgm one that 4 qod Wco D sabe Tlle sas the iniu Twnle T, ia T In Q 'q Te Te Te 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4

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  the content of the element in the sample to be analyzed.

  On the other hand, if the molded mixture of metal bodies is molded by plastic deformation, because the zones of segregation between the metal bodies are dispersed by undergoing the effect of plastic deformation until the phenomenon of segregation becomes hardly observable, such a standard sample can give a more accurate calibration curve as well as a more accurate drift correction, and, consequently, the content of the element in the sample can

  to be analyzed more precisely.

  we will now describe the process of preparing a

  sample standard according to the present invention.

  By metal body is meant, in the present invention, a fine powder, grains, a piece, a sheet, a rod, a thin wire, etc. Such a metal body can be obtained from a molded ingot prepared by a method for molding a metal in a matrix, an indirect cooling casting method of the water cast metal or a direct quenching casting process, by physically spraying the molded ingot, for example in a sprayer , or by rolling the ingot according to a sheet, a rod or a thin wire, followed by a sawing In addition, the metal body can

  also be prepared by chemical reaction.

  Mixing can be carried out using a common mixer, but it is more convenient for handling to mix and mold a single type of metal body with a

desired composition.

  Alternatively, it is also possible to mix and mold while combining metal bodies of different types such as powder and thin wire Not only the metal body of the same composition but also metal bodies of different compositions can be mixed and molded For example, in the case of the preparation of a standard sample of an alloy of the Al-Si-Cu-Mg series, a powder of an Al-Cu-Mg series alloy and a powder of a a Te In D Tpuad'ada; e kns au, n Lb Fr np alqeaagadd 4 uawao Tlzn D Tqajd qsa uo Tsnaxa, p anbtl; zaq e 'anb Tllaugw sdio;) lip abelnoul np sano D anib T-4 seld uo Lew Iojgp Pl Jaas T Iea lnod sapppojd sal Tl Iud D 4 a' abeablo; '5 abe 6 PUT Ti D SE

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  a high rate of plastic deformation.

  In this connection, the extrusion technique is particularly advantageous when the metal body consists of grains, powder, wire, rod, foil, etc. for the reasons indicated below. Moreover, the metal body can undergo plastic deformation by rolling, forging, etc. in addition to the extrusion In this case, since it is generally necessary to have a diameter allowing a number of analyzes within a sufficient portion of the same surface, namely With a diameter of about 40 to 60 mm, large scale fabrication is required to make the surface perpendicular to the flow of the metal greater than necessary to allow analysis. usually in the surface parallel to the flow of the metal In such a surface, since the metal body has an elongated constitution, the number of original metal bodies per unit area is r compared with the case of extrusion manufacturing and

  the homogeneity of the sample is somewhat deteriorated.

  However, if a small metal body is chosen, a much more homogeneous sample can be obtained in comparison with the conventional disk-shaped sample prepared by die casting or by casting.

  semi-continuous direct cooling.

  In the present invention, there is no particular restriction with regard to the composition of the metal body. For example, in the case of aluminum alloys, the invention makes it possible to obtain a quite excellent effect for an alloy of a composition containing elements such as Ti or Fe etc. that can be segregated during the solidification of the aluminum alloy beyond the peritectic point or the eutectic point, or alloys of the AI series -12 to 25% by weight of Si containing silicon capable of precipitating silicon primary crystals beyond the eutectic point The present invention obviously gives an excellent result also for aluminum alloys containing less than 12% by weight of Si De Moreover, the present invention can also give an excellent result for aluminum alloys containing Pb, Bi, etc. likely to cause severe segregation, for alloys of the Al-Ti series. -B likely to cause agglomeration of inter-metallic compounds, as well as for

  alloys of the Al-Cu-Mg series or Al-series alloys

  Cu-Mg-Zn containing Cu, Zn, Mg, etc. In the case of using optical emission spectrometry using a standard sample according to the present invention as the sample to be analyzed having a metallurgical hysteresis different from that of the sample conventional standard, since the spectral intensity ratio of silicon is different, even for an identical silicon content which is supposedly dependent on the size of the primary silicon crystals, it is necessary to first recognize the extent of this effect by a preliminary measurement and apply a correction (Japanese standard

JIS / H 1305).

  Other features and advantages of the present invention will now be described in more detail with reference to examples of the invention and with reference to the accompanying drawings in which: Figure 1 is a graph showing the analysis value and the deviation standard when the standard sample according to the present invention is subjected to optical emission spectrometry; Figures 2A and 2B are curves showing the analysis value and the standard deviation when the samples prepared by a matrix casting process are subjected to optical emission spectrometric analysis, and Figure 3 is a curve showing the value of analysis and standard deviation when a molded rod cast in a horizontal semi-continuous process is subject to

  to spectrometric analysis by optical emission.

EXAMPLE 1

  A JIS AC 9 B alloy (of composition: Al-18.9% by weight of Si 1.4% by weight of Cu 10% by weight of Mg 1.2% by weight of Ni 0.4% by weight of Fe calculated on the mixture) was prepared by melting at 8500 C and pulverized with a rotary perforated crucible to obtain a granular metal body with an average grain size of 0.8 mm ( grains between 0.3 and 3 mm) at a cooling rate of 102 103 OC / second The metal bodies were placed in a container with a bottom, having an internal diameter of 100 mm and a length of 150 mm and the The extruded cylindrical rod was cut into lengths of 50 mm in length and a surface perpendicular to the extrusion direction was machined to prepare specimens for extrusion.

  spectrometric analysis by optical emission.

  Optical emission spectrometry was performed in

the following conditions.

  Emission source: High voltage spark process Atmosphere: air Counter electrode: graphite rod Wavelength: Si 390.55 nm Al 256, 80 nm (internal standard) Element: Si Spark location: central part (inside

half a radius) and part of

external interface (location

equivalent to outside

half a radius) in an over-

  this perpendicular to the direction of extrusion every 50 mm in length. An analysis of each specimen was performed five times on the same surface. The results of the analysis are

shown in Figure 1.

  In FIG. 1, each of the points represents an average value for five analyzes. Moreover, the value of the standard deviation W n-1 for each group of five measurements for the central part and for the external peripheral part, ie 10 measurements in total. for each of the specimens was 0.11 to 0.16% by weight. According to the results of FIG. 1, the analysis value was between 18.7% and 19.0% by weight, the deviation of the analysis value depending on the locations of the sparks in the direction of extrusion depends little of the high silicon content and, in addition, the dispersion of the value of the standard deviation Tn-1 for the same area is small, between 0.11 and 0.16% by weight and, consequently, it can be seen that location-dependent segregation is low and specimens are suitable for a spectrochemical standard

  by optical emission for Al-Si hypereutectic alloys.

EXAMPLE 2

  The granular metal body according to Example 1 was compressed using a 600 ton press to obtain a rod 40 mm in diameter and 100 mm in length. The compressed rod was cut into sections of 50 mm in diameter. length and a face perpendicular to the longitudinal direction was cut to prepare a specimen for optical emission spectrometry The optical emission spectrometry was implemented according to the same procedure as in Example 1 According to the results of the analysis, the value average for the five points of the central portion was 18.8% by weight, the average value for the five points in the outer peripheral zone was 19.0% by weight and the value of the standard deviation T n- 1 for the ten points of sparks was 0.19% by weight. These results show that the deviation of the analysis value is small and that, in addition, the dispersion of the value of the deviation stallion n 1 in one the surface is weak, location-dependent segregation is low and the specimen is suitable as a standard for optical emission spectrochemical analysis for alloys

hypereutectic Al-Si.

COMPARATIVE EXAMPLE 1

  As a comparator, an alloy with a high silicon content (A 1 16.5% by weight of Si 4.7% by weight of Cu 0.55% by weight of Mg 0.3% by weight of Fe) and a low silicon content alloy (Al 14.6% by weight of if 0.46% by weight of Cu 0.5% by weight of Mg 0.3% by weight of Fe) (values calculated in the mixture) were 8000 C and A 390 0 AA (Aluminum Association) alloys and each was cast in a matrix having a disk-shaped cavity 55 mm in diameter and 10 mm deep, in order to The molded body thus obtained was machined on a surface perpendicular to the central axis and subjected to optical emission spectrometry. The area of sparks was determined in the outer circumferential part of the surface perpendicular to the axis. central The analysis of each specimen was carried out using five measurements on the same surface and such the measurements were repeated after cutting the specimen every millimeter The results of the analysis are shown in FIGS. 2A and 2B each of the points of FIG.

  average value of the five measures defined above.

  The analytical value for the high Si content alloy shown in Figure 2A was between 16.2 and 17.4% by weight and because segregation is important in the direction of thickness and that the value of the standard deviation T n-1 (n = 5) in the same area is between 0.18 and 0.47% by weight, it can be observed that site-dependent segregation is important and that the In addition, the analytical value for the low-content alloy as shown in FIG. 2B was between 14.2 and 15.0% by weight and because segregation in the thickness direction is important and the standard deviation r n-1 (n = 5) for the same area is between 0.12 and 0.31% by weight, it can be seen that that segregation is important depending on the locations and the body is not appropriate for

constitute a standard sample.

COMPARATIVE EXAMPLE 2

  As a comparison substance, an alloy A 390 9 according to the AA standard (A 1-15, 5% by weight of Si 4.7 by weight of Cu 0.55% by weight of Mg 0.3% by weight of Fe calculated in the mixture) was prepared by melting at 750 C Pt a casting rod

  58 mm in diameter was obtained by casting in half

  continuous The spark location for the cast rod has been fixed in the central zone (within half a radius) and in the outer peripheral part thereof (equivalent location outside a half-diameter) in a surface perpendicular to the direction of casting and the rod was cut 4 e every 1000 mm in the longitudinal direction The analysis of each specimen was conducted five times for the central part and for the outer peripheral part on the same surface

  The results of the analysis are shown in Figure 3.

  In Figure 3, each of the points represents an average value for five measurements. In addition, the value of the standard deviation q n-1 (11 = 10), for a total of ten measurements, namely, five for the central part and five for the outer peripheral part for each of the specimens, has been included

between 0.5 and 1.0% by weight.

  From the results of FIG. 3, the analysis value was between 15.0 and 16.2% by weight, the segregation depending on the locations of the sparks in the direction of casting is important and the standard deviation V 1 (= 10) to 1N the inside of the same area was between 0.5 and 1.0% by weight and it can be seen that the body is not suitable

  to constitute a standard sample.

  As mentioned above, since the content of the element is homogeneous and the quality is stable in the optical emission spectrochemistry standard for metals and alloys, in particular aluminum and its alloys, in accordance with In the present invention, the content of the element in the sample to be analyzed can be accurately analyzed and determined and, accordingly, the exact performance of the sample can be accurately predicted and recognized.

  various types of products or semi-products.

Claims (3)

R E V E N D I C A T IO N S   1 Spectrochemical optical emission test standard for metals and alloys, characterized in that it consists of   a melted mixture of small metal bodies.   2 standard according to claim 1, characterized in that the metal body comprises an aluminum alloy. 3. Standard according to claim 2, characterized in that the metal body contains between 12 and 25% by weight of silicon. 4 Standard according to claim 1, characterized in that the metal body is a product obtained by rapid solidification. Standard according to claim 1, characterized in that   the molded mixture undergoes a plastic deformation.   6 aluminum alloy standard according to claim 2 or 3, characterized in that it consists of a molten mixture of small bodies of aluminum alloys, in that the latter are products obtained by fast solidification and in that said molded mixture is subjected to plastic deformation.